Assxsboel



[Patented Sept-'2, i930 UNITEEYD STATES CHARLES E. BURKE, or WILMINGTON,nnr gew rm as:

ssmma r movns '& COMPANY, .orwnmmoron'fni "mam Arron Ola-Pozna- WARE 4PENTAER THRITE E'rHEasAND PROCESS or PREPARING KoDtawlng.

v151the wholemass in a nickel autoclave for approximately -eighthours,raising the temperature to about 150 C. in the course of two hoursand Inaintaining atahout 150 C. for the remainder of the tim'e. Thisreaction iscarried out at a pressure-of approximately -200-2l0'-pounds'persqu are inch. hen the reaction is completed. allow the mass to coolover nighhfilter, anddistill oil,

the iicnzine from the filtrate. Then fraciionate the-residualmaterialunder reduced pressure, takin; three fractions. The firstfraction distills atatemperature of 150""- 15sec.-n em-press mpf 44 'm'i. mercurv s awa er- Ira ta sale unden apressure mm, an'd-thethirdfraction at 2Q0-260 C. An analysis of these fractions indicates thatthefirst frac- 1 tion consists of approximately 80% triethyl ether and 20%diethyl ether; the second frac- 35 tion, -20- %"triethyl ether and 80%diethvl ether; and the-third fraction 87% dieth'yl ether, and 12%monoethyl-ether. 7 All threefractions are pale yellow oils and theviscosity ofthe' third fraction'is much 4 higher than that offractionsone and two.

In place of a chloride.,such as ethyl chloride, there may be used estersof other inorganic acids, for example, bromides, iodides, sulfates andthe like; 'andin place- 0f ethyl chloride there may be used esterscontaining Application filed January 27, 1928. Serial No.- 250,093.

other organic radicals, for eirample, methyl chloride, butyl chloride,benzyl chloride and the like.

These pentaerythrite ethers are, in general, .useful as solvents,softeners and plasticizers for cellulose derivatives, for example,cellulose ethers or for cellulose esters sue as-cellu- -'l0se nitrate,cellulose acetziteiand the like.

The following is one method suitable for pro ducing compositions of thisnature. Take 100 parts of a cellulose derivative, such as cellulosenitrate, and from'2to601parts of pentaeryth rite ether, for;eramplegthe"dieth'yl ethers,-'an'd to this addtafisufiic"int-quantity of"a mutual solventto forth .a plastic mass Such a composition'mgyxbg; lgtji gd i n:

mixer followed b'yrolling,cakepressing 'and sheeting, according to}'thefmethods' known to theplastic art,.or'the'compo'sition may bedissolved in a suitable volatile" solvent and. thinned to a'consistencysuitable for a'coating' composition with or without the addition ofoils, resin pigments and thelil se.

bodiments of this invention without depart mg from H19 to he "Anders-t dthat i do not limit myself As many apparently widely diiierent ema be,made 5 it thereof. it i il'qnthevfhumoiahe m-mplegsm description,

following patent claims.

I claim-: 1. The process of preparing pentaerythrite others whichcomprises heating an esterof an inorganic acid with pentaerythrite'underpressure in the presence offa solvent and an,-. alkali. and distillingoff the solvent.

2. The process of preparing pentziez vthrite ethers which comprisesheating a halogen ester with pentaezythrite under pressure 2r.-

the presence of a solvent and a1;- aikali, and.

distilling off the solvent.

3. The. process of preparing pentaei vthrite ethers which comprisesheatin an alkyl chloride with pentaerythrite un er pressure in thepresence of a solvent and an alkali, and distilling off the solvent. 4.The process of preparing pentaerythrite ethers which comprises heatingethyl chloride with pentaerythrite under pressure in the presence of asolvent and an alkali, and distilling off the solvent.

5. An alkyl ether of pentaerythrite having less than four alkyl groups.

6. An ethyl ether of pentaerythrite having less than four ethyl groups.

7. A diethyl ether of pentaerythrite:

In testimony whereof I afiix my signature.

- CHARLES E. BURKE.

